Synthesis and Structural Characterization of ... - Jacobs University

More documents

Recommendations

Info

Chapter 3 Unpublished Results Na 8 [Yb 2 (H 2 O) 6 (Sb 2 W 20 O 70 )]·37H 2 O (Na-18) 0.068 g (0.175 mmol) of YbCl 3·6H 2 O was added to 20 mL 1M NaCl (aq) with stirring followed by addition of 0.50 g (0.175 mmol) of Na 9 [B-α-SbW 9 O 33 ]·19.5H 2 O, and then the pH was adjusted to 4.8 with 2M HCl. The solution was stirred at 50 ˚C for 30 min, allowed to cool to room temperature. The filtrate was kept in an open vial for crystallization. After about a week colorless crystals were obtained, which were filtered off and air dried (yield 0.24 g, 43 %). IR for Na-18 showed metal-oxygen stretches at 951(s), 862(sh), 821(s), 771(m), 646(m), 527(w), 513(w), 494(w), 468(m), 421(m), 418(m) cm -1 (see Figure 3.28). Anal. Calcd for Na-18: Na, 2.9; Sb, 3.8; W, 57.9; Yb, 5.5. Found: Na, 2.4; Sb, 3.8; W, 56.0; Yb, 7.9. Therefore, the elemental analysis suggests the following formula: Na 6.5 Yb 0.5 [Yb 2 (H 2 O) 6 (Sb 2 W 20 O 70 )]·37H 2 O. Na 8 [Lu 2 (H 2 O) 6 (Sb 2 W 20 O 70 )]·38H 2 O (Na-19) The same procedure as Na-18 was followed, except for using 0.068 g LuCl 3·6H 2 O. Yield: 0.20 g (35 %). IR data for Na-19: 951(s), 862(sh), 821(s), 771(m), 646(m), 527(w), 513(w), 494(w), 468(m), 421(m), 418(m) cm -1 (see Figure 3.28). Anal. Calcd for Na-19: Na, 3.5; Sb, 3.8; W, 59.5; Lu, 2.7. Found: Na, 2.4; Sb, 3.8; W, 58.6; Lu, 3.2. Na 8 [Y 2 (H 2 O) 6 (Sb 2 W 20 O 70 )]·37 H 2 O (Na-20) The same procedure as Na-18 was followed, except for using 0.044 g YCl 3·6H 2 O. Yield: 0.21 g (39 %). IR data for Na-20: 951(s), 862(sh), 821(s), 771(m), 646(m), 527(w), 513(w), 494(w), 468(m), 421(m), 418(m) cm -1 (see also Figure 3.28). Anal. Calcd for Na-20: Na, 2.98; Sb, 4.0; W, 59.5; Y, 2.9. Found: Na, 2.6; Sb, 4.1; W, 60.1; Y, 4.1. Therefore, the elemental analysis suggests the following formula: Na 6.5 Y 0.5 [Y 2 (H 2 O) 6 (Sb 2 W 20 O 70 )]·37 H 2 O. Elemental analyses were carried out by Zentralabteilung für chemische Analysen, Forschungszentrum Jülich GmbH, Jülich, Germany. 119
Chapter 3 Unpublished Results Figure 3.28. IR spectra of the three compounds Na-18 (pink line), Na-19 (balck line), and Na-20 (green line) (from bottom to top). 3.B.2.3. X‐ray Crystallography The crystallographic data are summarized in Table 3.5 and 3.6. 120
Page 1 and 2:
Synthesis and Structural Characteri
Page 3 and 4:
Amal H. Ismail Ph.D. Thesis Acknowl
Page 5 and 6:
Amal H. Ismail Ph.D. Thesis Abstrac
Page 7 and 8:
Amal H. Ismail Ph.D. Thesis 1.6.1 P
Page 9 and 10:
Amal H. Ismail Ph.D. Thesis 3.B.1.2
Page 11 and 12:
Amal H. Ismail Ph.D. Thesis 5.B.2.
Page 13 and 14:
Amal H. Ismail Ph.D. Thesis Figure
Page 15 and 16:
Amal H. Ismail Ph.D. Thesis (pink);
Page 17 and 18:
Page 19 and 20:
Page 21 and 22:
Amal H. Ismail Ph.D. Thesis List of
Page 23 and 24:
Amal H. Ismail Ph.D. Thesis K 8 Cs
Page 25 and 26:
Chapter 1 Introduction proposed a s
Page 27 and 28:
Chapter 1 Introduction A or B. At s
Page 29 and 30:
Chapter 1 Introduction c) [(H 2 )W
Page 31 and 32:
Chapter 1 Introduction by protonati
Page 33 and 34:
Chapter 1 Introduction structures;
Page 35 and 36:
Chapter 1 Introduction mono-, di-,
Page 37 and 38:
Chapter 1 Introduction Removal of t
Page 39 and 40:
Chapter 1 Introduction α-[P 2 W 18
Page 41 and 42:
Chapter 1 Introduction Figure 1.10
Page 43 and 44:
Chapter 1 Introduction In general,
Page 45 and 46:
Chapter 1 Introduction 1.6.1 Photoc
Page 47 and 48:
Chapter 1 Introduction dioxygen is
Page 49 and 50:
Chapter 1 Introduction 1.7 Lanthani
Page 51 and 52:
Chapter 1 Introduction ligand for o
Page 53 and 54:
Chapter 1 Introduction [Gd 8 As 12
Page 55 and 56:
Chapter 1 Introduction Recently, we
Page 57 and 58:
Chapter 1 Introduction P 2 W 16 O 5
Page 59 and 60:
Chapter 1 Introduction [7] L. C. Pa
Page 61 and 62:
Chapter 1 Introduction Malacria, C.
Page 63 and 64:
Chapter 1 Introduction [55] B. Nohr
Page 65 and 66:
Chapter 2 Experimental 2.2 Instrume
Page 67 and 68:
Chapter 2 Experimental 2.3.2 Synthe
Page 69 and 70:
Chapter 2 Experimental 2.3.8 Synthe
Page 71 and 72:
Chapter 2 Experimental 2.4 Referenc
Page 73 and 74:
Chapter 3 Published Results general
Page 75 and 76:
Chapter 3 Published Results 2.5 mL
Page 77 and 78:
Chapter 3 Published Results Na 8 [T
Page 79 and 80:
Chapter 3 Published Results matrix
Page 81 and 82:
Chapter 3 Published Results 3.A.1.4
Page 83 and 84:
Chapter 3 Published Results [H 2 W
Page 85 and 86:
Chapter 3 Published Results and one
Page 87 and 88:
Chapter 3 Published Results {W 4 }
Page 89 and 90:
Chapter 3 Published Results We also
Page 91 and 92: Chapter 3 Published Results Figure
Page 93 and 94: Chapter 3 Published Results We trie
Page 95 and 96: Chapter 3 Published Results M. T. P
Page 97 and 98: Chapter 3 Published Results 72.936(
Page 99 and 100: Chapter 3 Published Results La, Ce,
Page 101 and 102: Chapter 3 Published Results Na 8 Eu
Page 103 and 104: Chapter 3 Published Results Table 3
Page 107 and 108: Chapter 3 Published Results Polyani
Page 109 and 110: Chapter 3 Published Results [LnW 10
Page 111 and 112: Chapter 3 Published Results analogu
Page 113 and 114: Chapter 3 Published Results We also
Page 115 and 116: Chapter 3 Published Results example
Page 117 and 118: Chapter 3 Published Results 1737; q
Page 119 and 120: Chapter 3 Published Results 3.B. La
Page 121 and 122: Chapter 3 Published Results expecte
Page 123 and 124: Chapter 3 Published Results 3.B.1.3
Page 127 and 128: Chapter 3 Published Results differe
Page 133 and 134: Chapter 3 Published Results Acta 20
Page 135 and 136: Chapter 3 Published Results Chem.,
Page 137 and 138: Chapter 3 Unpublished Results bond
Page 139 and 140: Chapter 3 Unpublished Results lanth
Page 141: Chapter 3 Unpublished Results Na 10
Page 145 and 146: Chapter 3 Unpublished Results 3.B.2
Page 147 and 148: Chapter 3 Unpublished Results In po
Page 149 and 150: Chapter 3 Unpublished Results Figur
Page 153 and 154: Chapter 3 Unpublished Results (a) (
Page 155 and 156: Chapter 3 Unpublished Results param
Page 157 and 158: Chapter 3 Unpublished Results G.-F.
Page 159 and 160: Chapter 3 Unpublished Results Here
Page 163 and 164: Chapter 3 Unpublished Results This
Page 165 and 166: Chapter 3 Unpublished Results techn
Page 169 and 170: Chapter 4 Unpublished Results Chapt
Page 171 and 172: Chapter 4 Unpublished Results The c
Page 173 and 174: Chapter 4 Unpublished Results iron(
Page 175 and 176: Chapter 4 Unpublished Results 4.4.
Page 181 and 182: Chapter 4 Unpublished Results Therm
Page 183 and 184: Chapter 4 Unpublished Results This
Page 185 and 186: Chapter 4 Unpublished Results 4.6.
Page 187 and 188: Chapter 4 Unpublished Results S. Ba
Page 189 and 190: Chapter 5 Published Results Also te
Page 191 and 192: Chapter 5 Published Results 5.A.1.3
Page 193 and 194:
Chapter 5 Published Results Table 5
Page 195 and 196:
Chapter 5 Published Results [HTe 2
Page 197 and 198:
Chapter 5 Published Results face-sh
Page 199 and 200:
Chapter 5 Published Results polymol
Page 201 and 202:
Chapter 5 Published Results Each of
Page 203 and 204:
Chapter 5 Published Results Althoug
Page 205 and 206:
Chapter 5 Published Results Polyako
Page 207 and 208:
Chapter 5 Unpublished Results 5.A.2
Page 209 and 210:
Chapter 5 Unpublished Results 610(m
Page 211 and 212:
Chapter 5 Unpublished Results 5.A.2
Page 213 and 214:
Chapter 5 Unpublished Results Figur
Page 215 and 216:
Chapter 5 Unpublished Results {Mo 6
Page 217 and 218:
Chapter 5 Unpublished Results compo
Page 219 and 220:
Chapter 5 Unpublished Results [3] a
Page 221 and 222:
Chapter 5 Published Results 5.B. Tr
Page 223 and 224:
Chapter 5 Published Results H 2 O)
Page 225 and 226:
Chapter 5 Published Results 5.B.3.
Page 227 and 228:
Chapter 5 Published Results Each Ke
Page 229 and 230:
Chapter 5 Published Results GeW 9 O
Page 231 and 232:
Chapter 5 Published Results the axi
Page 233 and 234:
Chapter 5 Published Results The man
Page 235 and 236:
Chapter 5 Published Results 5.B.6.
Page 237 and 238:
Chapter 5 Published Results [19] L.
Page 239:
Amal H. Ismail Ph.D. Thesis Appendi
show all

Synthesis and Structural Characterization of ... - Jacobs University

You also want an ePaper? Increase the reach of your titles

Delete template?

Save as template?